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1.
Using LC–MS/MS, a rapid and sensitive method for the simultaneous determination of pyraclostrobin and azoxystrobin residues in banana matrices (leaf and whole banana) and soil was established. The samples were extracted using acetonitrile and purified through C18 dispersive solid-phase extraction. The average recovery of the analytes in various matrices was in the range of 77.3%–103.9% with an RSD range of 0.9%–9.5%. The initial deposition amounts of pyraclostrobin and azoxystrobin at 2 h in the banana leaves of the mineral oil group were 1.43 and 1.31 times in Guangxi, and 2.10 and 1.81 times in Hainan for the water group, whereas those in the soil of the water group were 3.45 and 3.03 times in Guangxi, and 2.14 and 3.48 times in Hainan for the mineral oil group. The half-lives in the leaves and soil of the mineral oil group were not remarkably different from those of the water group. The terminal residue of the analytes on the whole banana was <0.02 mg/kg at 14 days after application from the two sites. The results of this work may indicate and promote the safety of using pyraclostrobin and azoxystrobin in banana production, especially with mineral oil spray adjuvants.  相似文献   

2.
The dissipation dynamics and final residues of flutriafol on tobacco plant and soil were studied under field conditions. The residues of flutriafol in soil, green tobacco leaves and cured tobacco leaves were extracted by ultrasound-assisted extraction, cleaned up by dispersive solid-phase extraction and detected by liquid chromatography with tandem mass spectrometry. The limits of detection of flutriafol in soil, green tobacco leaves and cured tobacco leaves were 0.006, 0.033 and 0.033 mg·kg?1, respectively. The limits of quantification of flutriafol in soil, green tobacco leaves and cured tobacco leaves were 0.02, 0.1 and 0.1 mg·kg?1, respectively. Recoveries were 72.9–102% with relative standard deviations of less than 12% in soil and tobacco matrix. For field experiments, the half-lives of flutriafol in soil and green tobacco leaves were 9.2–11.5 and 9.5–11.1 days, respectively. At harvest, the final residue levels of flutriafol in cured tobacco leaves collected 21 days after one application at the recommended dosage were below 2.0 mg/kg. The maximum residue limit maximum residue limit (MRL) for flutriafol in tobacco has not yet been established in any countries. The data could help the Chinese Government to establish the MRL of flutriafol in tobacco and provide guidance on the proper use of flutriafol.  相似文献   

3.
Trifloxystrobin and tebuconazole are used for control of Sigatoka leaf spot disease of banana. This study was conducted to evaluate residue persistence of the fungicides in/on banana fruit, other edible parts and soil after spray application of the combination formulation, Nativo 75 WG, at the standard dose, 87.5 + 175 and double dose, 175 + 350 g a.i. ha?1. The fungicides were extracted from banana and soil with acetone, partitioned into dichloromethane and cleaned-up using activated charcoal for trifloxystrobin and primary/secondary amine (PSA) for tebuconazole samples. The limit of quantification of the method was 0.05 mg kg?1 for both fungicides. Initial residues of trifloxystrobin were 0.444 and 0.552 mg kg?1 in/on banana with peel (whole fruit), which reached <0.05 and 0.065 mg kg?1 after 30 days from treatment at the standard and double doses, respectively. Tebuconazole residues were 0.636 and 960 mg kg?1 initially and reduced to 0.066 and 0.101 mg kg?1 after 30 days. Trifloxystrobin and tebuconazole degraded with the half-life of about 11 days. Trifloxystrobin or its metabolite was not detected in the fruit pulp. Tebuconazole being systemic in nature moved to the fruit pulp which was highest on the 3rd day (0.103 and 0.147 mg kg?1) and remained for 15 days. Matured banana fruit, flower, pseudostem and field soil were free from fungicide residues. For consumption of raw banana 43 days pre-harvest interval (PHI) is required after treatment of the combination formulation. Therefore application of the fungicides towards maturity stage of the fruits may be avoided.  相似文献   

4.
A method based on QuEChERS-like extraction and UPLC-ESI-MS/MS for the analysis of flonicamid was established. The samples were extracted by acetonitrile–methanol mixture and were purified using PSA. At fortification levels of 0.01, 0.1 and 0.5 mg/kg in cucumber, apple and soil, recoveries ranged from 71.5 to 106.0% with relative standard deviation (RSD) of 2.6–9.9%. The limit of quantification (LOQ) was 0.003 mg/kg for cucumber, apple and soil. This study also investigates the dissipation of flonicamid in cucumber, apple and soil. The dissipation half-lives of flonicamid in cucumber, apple and soil were 3.0–4.9 days, 5.1–6.1 days and 10.3–14.2 days, respectively. The final residues of flonicamid ranged from 0.029 to 0.295 mg/kg in cucumbers, <0.01–0.174 mg/kg in apples and <0.01–0.172 mg/kg in soil, respectively. The observed low residual levels of flonicamid suggest that the cucumber and apple are safe when applied at the recommended dosage.  相似文献   

5.
A field experiment was conducted to evaluate clofentezine residue levels and dissipation trend in tangerine and soil for the safe application of clofentezine. A modified QuEChERS-HPLC-UVD method was developed to analyse clofentezine in tangerine and soil. Tangerine samples were homogenised and extracted by acetonitrile and then cleaned up with dispersive solid phase extraction (dSPE) by primary and secondary amine (PSA) and C18. Clofentezine residue was determined by high-performance liquid chromatography (HPLC) with a UV detector (UVD) at the wavelength of 268 nm. The presented method achieved the good linear relationship within the range from 0.05 to 5.0 mg kg?1 for clofentezine (R2 > 0.998). At the fortification levels of 0.05, 0.50 and 1.00 mg kg?1 in tangerine pulp, tangerine peel and soil, recoveries ranged from 75.9% to 117.7% with relative standard deviations (RSD) less than 8.2%. In the supervised field trials, the half-lives of clofentezine in tangerine and soil were approximately 11.3 and 8.6 days, respectively. At pre-harvest interval of 21 days, the residue of clofentezine in tangerine was below the maximum residue limits (MRL) (0.5 mg kg?1). Clofentezine (Water Dispersible Granule, 80%) was recommended to be sprayed twice and the recommended dosage ranged from 250 to 375 mg kg?1.  相似文献   

6.
In this study, a rapid and sensitive method was developed for determining fenamidone and propamocarb hydrochloride residues in vegetables and soil by ultra-performance liquid chromatography-tandem mass spectrometry. The dissipation dynamics of fenamidone and propamocarb hydrochloride in pepper and soil was investigated in Beijing, Henan and Shandong provinces. The target compounds were extracted with methanol and cleaned with dispersive solid phase extraction using primary secondary amine. Two pairs of precursor product ion transitions for fenamidone and propamocarb hydrochloride were measured and evaluated. Average recoveries of fenamidone in potato, tomato, cabbage, pepper and soil at three levels (10, 100 and 1000 μg kg?1) ranged from 76.91% to 107.31% with relative standard deviations (RSDs) from 2.74% to 10.87% (n = 15). The average recoveries of propamocarb hydrochloride ranged from 74.84% to 97.96% with RSDs from 2.43% to 16.16% (n = 15). The limits of detection (LODs) for fenamidone in each matrix were 0.131–0.291 μg kg?1, and the limits of quantification (LOQs) were 0.436–0.970 μg kg?1. The LODs for propamocarb hydrochloride were 0.125–0.633 μg kg?1, and the LOQs were 0.417–2.11 μg kg?1. The results also showed that the dissipation of fenamidone and propamocarb hydrochloride in pepper and soil followed first-order kinetics model more than that of bi-exponential models. The half-lives of propamocarb hydrochloride were 6.90–15.78 days in pepper and 13.56–23.02 days in soil. The half-lives of fenamidone were 7.48–11.29 days in pepper and 35.18–42.78 days in soil.  相似文献   

7.
The combinational fungicide suspension (11.7% propiconazole + 7% azoxystrobin), developed by Syngenta Co., Ltd., is very effective for the control of Alternaria black spot on ginseng. A simple and effective method was developed for determining propiconazole and azoxystrobin residues by high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The recoveries of propiconazole ranged from 81.0% to 98.0% with relative standard deviations (RSDs) of 1.23–8.46%, while the recoveries of azoxystrobin ranged from 83.2% to 98.8% with RSDs of 3.29–9.50%. For the dissipation kinetics, the combinational fungicide was sprayed with dosage of 225 g a.i.ha?1 (1.5 times of recommended dosage) in ginseng and soil at two different locations. The dissipation kinetics followed the first-order kinetics with half-lives of 6.66–13.33 days for propiconazole and 4.92–9.12 days for azoxystrobin. Based on the terminal residues data, the preharvest interval (PHI) could be 35 days at recommended dosage in ginseng. The dietary exposure risk was estimated by risk quotient (RQ). The result showed that the RQ value was obviously lower than RQ = 1, indicating that spraying propiconazole and azoxystrobin in ginseng at recommended dosage was safe for human beings.  相似文献   

8.
A modified QuEChERs method with liquid chromatography-tandem mass spectrometry for analysis of guadipyr residue and dissipation in rice matrices, paddy soil and paddy water was developed and validated. Mean recoveries and relative standard deviations in paddy soil, paddy water, rice plant, rice straw, rice hull and husked rice matrices at three spiking levels were 83.1–116.5% and 1.6–9.5%, respectively. The half-life of guadipyr was determined in 2 years at three different field sites in China via a dissipation experiment. The half-lives of guadipyr in paddy water were 0.22–0.37 days, 0.24–3.33 days in paddy soil and 0.44–1.90 days in rice plant. The terminal residues of guadipyr ranged from ND (concentrations of guadipyr were below limit of detection) to 50 μg kg?1 in paddy soil, 10–470 μg kg?1 in rice hull, ND70 μg kg?1 in husked rice and ND to 110 μg kg?1 in rice straw. The results would be helpful in fixing maximum residue limit of guadipyr, a new insecticide, in rice.  相似文献   

9.
Two independent field trials were performed in Guizhou and Hunan, China in 2013 to investigate the dissipation and residue levels of saisentong in tobacco and soil. A novel and accurate method using high-performance liquid chromatography with diode array detection was developed and validated to determine saisentong levels in tobacco and soil. The average recovery of saisentong at fortification levels of 0.5, 2.5, 5.0 and 50.0 mg kg?1 in fresh tobacco ranged from 75.92 to 107.40% with a relative standard deviation (RSD) of 0.94 to 7.55%, that at fortification levels of 0.5, 2.0 and 5.0 mg kg?1 in tobacco powder ranged from 74.96 to 94.43% with a relative standard deviation (RSD) of 4.38 to 8.14%, and that at fortification levels of 0.1, 0.5 and 5.0 mg kg?1 in soil ranged from 86.90 to 100.0% with an RSD of 1.38 to 4.62%. The limit of detection (LOD) of saisentong was 0.15 mg?kg?1 in tobacco and 0.03 mg kg?1 in soil, and the limit of quantification (LOQ) was 0.5 mg kg?1 in tobacco and 0.1 mg kg?1 in soil, respectively. For field experiments, the half-lives of saisentong in tobacco from Guizhou and Hunan were 5.9 and 1.6 days, respectively; those in soil were 14.7 and 12.0 days, respectively. The results suggest that the saisentong dissipation curves followed the first-order kinetic. The terminal residues of saisengtong in tobacco ranged from 0.5 to 9.39 mg kg?1 at pre-harvest intervals (PHI) of 7, 14 and 21 days.  相似文献   

10.
An optimized quick, easy, cheap, effective, rugged and safe method for the simultaneous determination of difenoconazole, trifloxystrobin and its metabolite trifloxystrobin acid residues in watermelon and soil was developed and validated by gas chromatography with tandem mass spectrometry. The samples were extracted with acetonitrile (1% formic acid) and cleaned up by dispersive solid‐phase extraction with octadecylsilane sorbent. The limit of quantification of the method was 0.01 mg/kg, and the limit of detection was 0.003 mg/kg for all three analytes. The recoveries of the fungicides in watermelon, pulp and soil were 72.32–99.20% for difenoconazole, 74.68–87.72% for trifloxystrobin and 78.59–92.66% for trifloxystrobin acid with relative standard deviations of 1.34–14.04%. The dissipation dynamics of difenoconazole and trifloxystrobin in watermelon and soil followed the first‐order kinetics with half‐lives of 3.2–8.8 days in both locations. The final residue levels of difenoconazole and trifloxystrobin were below 0.1 mg/kg (maximum residue level [MRL] set by China) and 0.2 mg/kg (MRL set by European Union), respectively, in pulp samples collected 14 days after the last application. These results could help Chinese authorities to establish MRL of trifloxystrobin in watermelon and provide guidance for the safe and proper application of both fungicides on watermelon.  相似文献   

11.
A high-performance liquid chromatography with ultraviolet (HPLC-UV) detection method after derivatisation was developed for the first time for the novel fungicide zinc thiazole residue in tobacco samples. Field trials in two different locations were conducted to investigate the dissipation and residue of zinc thiazole in tobacco leaves and soil. The average recoveries of zinc thiazole were in the range of 82.5%–93.9% with relative standard deviations (RSDs) of 1.2%–9.1%. The zinc thiazole showed a rapid dissipation rate in fresh tobacco leaves with the half-lives of 1.1–1.6 days. The terminal residues of zinc thiazole in cured tobacco leaves and soil were 2.8–28.0 mg kg?1and <0.05 mg kg?1, respectively. The results could be used to establish the maximum residue limits (MRLs) and provide guidance for the scientific use of zinc thiazole in agriculture.  相似文献   

12.
Chlorothalonil and azoxystrobin, as efficient and broad-spectrum fungicides, are two widely used fungicides to control downy mildew and anthracnose on cabbage. For the safe and rational use of these two pesticides on cabbage, their residues and dissipation were studied under field conditions. The trial results showed that chlorothalonil and azoxystrobin residues were affected by the frequency and dosage of application, and the weather condition post-application. Chlorothalonil and azoxystrobin dissipated rapidly in cabbage with the mean half-live of 1.7 and 0.4 days at three geographical experimental plots in China, respectively. The terminal residues of chlorothalonil and azoxystrobin in cabbage at harvest time were all below the maximum residue limit (MRL, 6 mg kg?1 for chlorothalonil and 5 mg kg?1 for azoxystrobin) established by Codex Alimentarius Commission. It suggested that this formulation of chlorothalonil and azoxystrobin (560 g L?1, SC) may be safer under the recommended dosage. Given that in China no MRL has been set for chlorothalonil and azoxystrobin in cabbage, this study could provide a guidance for establishing MRL, and the safe and rational use of these two pesticides.  相似文献   

13.
A modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the analysis of triallate residue in wheat and soil was developed and validated. Multi-walled carbon nanotubes were used as clean-up sorbent. The residual levels and dissipation rates of triallate in wheat and soil were determined by liquid chromatography–tandem mass spectrometry. The limit of quantification was established as 0.01, 0.02 and 0.05 mg kg?1 for soil, wheat and wheat plant samples, respectively. The average recoveries of triallate ranged from 77% to 108% at fortified levels of 0.01–0.5 mg kg?1 with relative standard deviations of 3.0–8.4% (n = 5). From residue trials at three geographical experimental plots in China, the results showed that the half-lives of triallate in soils were 1.13–1.63 days. For trials applied according to the label recommendation, the final residues of triallate in wheat at harvest time were all below 0.05 mg kg?1 (the maximum residue levels of China, Japan, Korea and the US).  相似文献   

14.
Dissipation and residue levels of bifenthrin and chlorfenapyr in eggplant and soil under field conditions were investigated using gas chromatography coupled with an electron capture detector (GC-ECD). The mean recoveries of bifenthrin and chlorfenapyr were 85.2–104.9%, with relative standard deviations (RSDs) of 0.5–9.1%. The limit of quantification (LOQ) was 0.01 mg kg?1. Bifenthrin exhibited half-lives of 3.3 to 4.1 days in eggplant and 17.8 to 25.7 days in soil; the half-lives of chlorfenapyr were 3.5 to 3.8 days in eggplant and 21.7 to 27.7 days in soil. During harvest, the terminal residues of bifenthrin and chlorfenapyr were below 0.031 and 0.083 mg kg?1, respectively. Risk assessment for different groups of people in China was evaluated. The risk quotients (RQs) of bifenthrin and chlorfenapyr were ranged from 0.0068 to 0.0148 and from 0.0033 to 0.0072, respectively. These results may provide guidance on reasonable use of pesticides and serve as a basis for establishing maximum residue limits (MRLs) in China.  相似文献   

15.
建立了低温冷冻液液萃取(LTF-LLE)/GC-MS结合保留指数对香蕉果肉及果皮中挥发性成分进行分析的方法,采用低温冷冻液液萃取对香蕉样品中的挥发性成分进行提取。分别鉴定出香蕉果肉及果皮中含有39种和32种挥发性成分,其主要成分为酯类物质。果肉果皮所含的挥发性成分在种类及相对含量上有一定差异,果肉中含量较高的组分为丙酸乙酯(11.88%)、乙酸异戊酯(9.45%)、棕榈酸(8.71%)、丁酸异戊酯(7.79%)、乙酸仲戊酯(5.29%),果皮中含量较高的组分为丁酸异戊酯(22.85%)、棕榈酸(15.91%)、硬脂酸(6.86%)、4-烯丙基-2,6-二甲氧基苯酚(6.83%)、亚麻酸(6.34%),果肉果皮所共有的成分有异戊醇、乙酸异丁酯、丁酸、异戊酸、乙酸仲戊酯等19种物质。  相似文献   

16.
A liquid chromatography–electrospray ionization tandem mass spectrometry method was developed for simple and accurate detection of the fungicides difenoconazole, propiconazole and pyraclostrobin in peppers and soil. Three fungicides residues were extracted from samples by acetonitrile and cleaned up by dispersive solid‐phase extraction before instrumental analysis. The accuracy and precision of the method were evaluated by conducting an intra‐ and inter‐day recovery experiment. The limits of quantification and detection of difenoconazole, propiconazole and pyraclostrobin in pepper and soil were 0.005 and 0.0015 mg/kg, respectively. The recoveries were investigated by spiking pepper and soil at three levels, and were found to be in the ranges 79.62–103.15% for difenoconazole, 85.94–103.35% for propiconazole and 80.14–97.69% for pyraclostrobin, with relative standard deviations <6.5%. Field experiments were conducted in three locations in China. The half‐lives of difenoconazole, propiconazole and pyraclostrobin were 5.3–11.5 days in peppers and 6.1–32.5 days in soil. At harvest, pepper samples were found to contain difenoconazole, propiconazole and pyraclostrobin well below the maximum residue limits of European Union at the interval of 21 days after last application following the recommended dosage.  相似文献   

17.
A rapid, highly sensitive, and selective method was developed for the determination of the insecticide chlorantraniliprole (CAP) in corn and soil using ultra-performance liquid chromatography?Ctandem mass spectrometry (UPLC?CMS/MS). Samples were extracted with acetonitrile, and aliquots were cleaned with solid-phase extraction cartridges. Two precursor-product ion transitions for CAP were measured and evaluated to provide maximum confidence in the results. Average recovery for soil, corn grain, and corn straw at different levels (5 or 10, 40, and 100 ??g kg?1) ranged from 74.9 to 97.5%, with intra-day relative standard deviation (RSD) values of 1.9?C11.3% and inter-day RSD values of 4.7?C10.4%. Coefficients of determination (R 2) of 0.9988 or higher were achieved for CAP in soil, corn grain, and corn straw matrix calibration curves, from 5 to 1,000 ??g L?1. The CAP limits of quantitation in soil, corn grain, and straw were determined to be 5, 10, and 10 ??g kg?1, respectively, which were much lower than the maximum residue levels established by the Environmental Protection Agency of United States. UPLC?CMS/MS was used to determine the CAP residues in real corn and soil for studies on their dissipation. The trial results showed that the half-lives of CAP changed from 12.6 to 23.1 days in soils and ranged from 4.9 to 5.4 days in corn straws in the districts of Henan and Shandong, and the average levels of CAP residues in corn grains were all <0.01 mg kg?1 with a harvest withholding period of 180 days.  相似文献   

18.
The chemical fungicide fludioxonil is widely used to control post-harvest fungal disease in cherries. This study was implemented to investigate the dissipation behaviours and residues of fludioxonil on cherries. A reliable and efficient analytical method was established. Cherry samples from four product areas were analyzed by QuEChERS and HPLC-MS/MS methods with acceptable linearity (R2 > 0.99), accuracy (recoveries of 81–94%), and precision (relative standard deviation of 2.5–11.9%). The limits of quantification (LOQs) and limits of detection (LODs) of cherries were 0.01 mg/kg and 0.005 mg/kg. The dissipation of fludioxonil on cherries followed first order kinetics with half-lives of 33.7–44.7 days. The terminal residues of fludioxonil were all lower than 5.00 mg/kg, which is the MRL recommended by the European Commission. According to Chinese dietary patterns and terminal residue distributions, the risk quotient (RQs) of fludioxonil was 0.61%, revealing that the evaluated cherries exhibited an acceptably low dietary risk to consumers.  相似文献   

19.
To investigate the dissipation rate of trinexapac-ethyl and trinexapac in wheat ecosystem, field and microbial degradation experiments were designed and conducted. A simple and time-efficient analytical method for the determination of trinexapac-ethyl and trinexapac in wheat kernels, plants, straw and soil, using high-performance liquid chromatography–tandem mass spectroscopy (HPLC–MS/MS) was developed. The mean recoveries of trinexapac-ethyl and trinexapac in four matrices at three spiking levels ranged from 72.0% to 108.2%, and the relative standard deviation (RSD) ranged from 2.1% to 11.0%. In supervised field trials, the half-lives of trinexapac-ethyl in the plants were 0.93 and 2.36 d in Shandong and Tianjin, respectively; and those of trinexapac in soil and plants were 1.66 and 1.45 d in Shandong and 2.32 and 1.74 d in Tianjin. In microbial degradation experiment, the results show that the soil microbial communities have effects on their dissipation in the time scale employed.  相似文献   

20.
The neonicotinoid imidacloprid is a very important insecticide in maize cultivation in China. A laboratory experiment was conducted to investigate its absorption, transportation and distribution in maize plants. Plants were exposed to an aqueous solution of imidacloprid at five concentrations (10, 20, 50, 100 and 200 μg/mL). The residues of imidacloprid in different plant parts were determined by using a quick and effective method of high-performance liquid chromatography. Results showed that the average recoveries ranged from 85.16% to 102.23%, with relative standard deviations of 1.82–4.40% at three different spiking levels in each different matrix. The half-lives of imidacloprid in hydroponic maize water were from 5.33 to 11.55 days. The concentrations in roots, stems and leaves were from 5.61 to 7.48, 1.03 to 4.03 and 0 to 30.57 μg/mL after 6 h–7 days exposed in 10 μg/mL imidacloprid aqueous solutions, respectively. Our study showed that imidacloprid was strongly absorbed by roots and mainly accumulated in leaves. Quantity ratio and bioconcentration factors (BCFs) were also used to estimate the distribution and accumulation in maize. The values of quantity ratios were the highest in the leaves while lowest in the root after 7 days treatments, with the ranking of leaves > stem > root. The BCFs were 0.63–1.66, 0.52–0.92 and 3.20–6.78 in root, stem and leaves, respectively. These results demonstrated that the exposed time and imidacloprid application concentrations were also the main factors influencing the absorption. This study enhances our understandings of the uptake and distribution of imidacloprid in maize plants.  相似文献   

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